Water → 4-(2-Bromofuran-3-yl)-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole

HRID 1274357ノート

反応式

HRID 1274357 の反応式
[C:1]([C:3]1[C:7]([C:8]2[CH:12]=[CH:11][O:10][CH:9]=2)=[CH:6][N:5]([C:13]2[C:18]([Cl:19])=[CH:17][C:16]([C:20]([F:23])([F:22])[F:21])=[CH:15][C:14]=2[Cl:24])[N:4]=1)#[N:2].[Br:25]N1C(=O)CCC1=O.CCOCC.O>O1CCCC1>[Br:25][C:9]1[O:10][CH:11]=[CH:12][C:8]=1[C:7]1[C:3]([C:1]#[N:2])=[N:4][N:5]([C:13]2[C:14]([Cl:24])=[CH:15][C:16]([C:20]([F:23])([F:21])[F:22])=[CH:17][C:18]=2[Cl:19])[CH:6]=1

参加物

6

反応物 4

HCID 962WaterHCID 3283Diethyl EtherHCID 67184N-bromobutanimideHCID 221208903-Cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-(furan-3-yl)pyrazole

生成物 1

HCID 98038424-(2-Bromofuran-3-yl)-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-(furan-3-yl)pyrazole (0.19 g) in tetrahydrofuran (5 ml) was added portionwise N-bromosuccinimide (0.093 g). The mixture was left at room temperature for 24 hours and then poured into ether (15 ml) and water (15 ml). The layers were separated and the organic layer was dried (Na2SO4) and evaporated. The residue was purified by column chromatography on silica gel (10 g) eluted with hexane:dichloromethane (1:1). Combination and evaporation of suitable fractions gave the title compound as a white solid, m.p. 111° C.

後処理

  1. customThe layers were separated
  2. dry with materialthe organic layer was dried (Na2SO4)
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel (10 g)
  5. washeluted with hexane:dichloromethane (1:1)
  6. customCombination and evaporation of suitable fractions

出典と根拠

ORDレコード
ord-e14dc681238648d88d6899185283153e
出典データセット
uspto-grants-2000_12
特許番号
US06156782

反応ノート

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